Organic silicon antireflection coating and preparation method thereof

Abstract

The invention belongs to the technical field of composite coatings, and particularly discloses an organic silicon antireflection coating and a preparation method thereof.The organic silicon antireflection coating composition is prepared from, by weight, 90-97 parts of epoxy organosilane; 0.2 to 3 parts of an alkane pore-foaming agent; 1-8 parts of a photoacid generator; and 0.25 to 0.5 part of an organic silicon leveling agent. The coating is coated on a substrate material, and the antireflection coating is obtained through light curing at a certain temperature. The coating is simple in formula, long in shelf life, low in cost and suitable for large-scale production, and the prepared coating material has the advantages of being high in light transmittance, low in reflectivity, good in mechanical strength and weather resistance and the like, can be widely applied to the fields of optical devices, photovoltaic cells, display screens and the like and is wide in market prospect.

Description

Technical Field

[0001] The invention belongs to the technical field of composite coatings, and in particular relates to an organosilicon anti-reflection coating and a preparation method thereof. Background Art

[0002] During the propagation of light, when the light enters from one medium to another, the different refractive indices of the two media cause the light to reflect at the interface between the two media. Studies have found that by using special coatings to apply a certain thickness of functional coating on the surface of the base material and using light interference to reduce light reflection, the light transmittance can be effectively improved. This type of functional coating can reduce the light reflection loss on the surface of the material and is usually called an anti-reflective coating or anti-reflective film. The corresponding special coating is called an anti-reflective coating, which has broad application prospects in photovoltaic solar cells, optical lenses, display screens and other fields.

[0003] Silicon-based coatings have attracted extensive attention in the field of optical coatings due to their excellent light transmittance, weather resistance, adhesion and mechanical strength. For example, Chinese patent CN110669362A discloses a weather-resistant closed-cell anti-reflective coating and its preparation method and use, which uses composite nanoparticles with a core-shell structure formed by spherical hyperbranched resin particles coated with network-shaped silicon oxide. After the coating is formed on the substrate and thermally cured, the core formed by the hyperbranched resin in the composite nanoparticles will be burned off (400°C to 700°C), leaving the hollow silicon oxide shell, i.e., hollow nanoparticles and the pore structure (i.e., gaps) between the hollow nanoparticles on the surface of the coating. The gaps between the hollow nanoparticles on the coating surface are filled with silicon oxide to form a closed-cell structure, thereby obtaining excellent anti-reflective performance. However, the coating formula is relatively complex, the added porous nanomaterials are difficult to disperse evenly, and a durable anti-reflective film can only be formed after being heated and cured at a certain temperature, which greatly restricts its industrial application. Summary of the invention

[0004] In view of the deficiencies of the prior art, the purpose of the present invention is to provide an organosilicon anti-reflection coating, the organosilicon anti-reflection coating of the present invention is coated on a substrate material, and the anti-reflection coating is photocured at a certain temperature to obtain the anti-reflection coating, and under ultraviolet light irradiation, a one-step polymerization method (hydrolysis, polycondensation of siloxane groups and cationic polymerization of epoxy groups) initiated by the decomposition of a photoacid generator to form a superacid is formed, and the formed organosilicon polymer is separated from the alkane phase, and a porous organosilicon polymer coating is formed after volatilization, and the film formed by self-assembly polycondensation has the characteristics of high light transmittance and good anti-reflection performance. The preparation process of the present invention is simple and efficient.

[0005] The present invention is achieved through the following technical solutions:

[0006] An organosilicon anti-reflection coating is formed by coating the organosilicon anti-reflection coating on a substrate material and then photocuring the coating. The organosilicon anti-reflection coating is composed of the following raw materials in parts by weight:

[0007] Epoxy organosilane 90-97 parts;

[0008] 0.2-3 parts of alkane porogen;

[0009] 1-8 parts of photoacid generator;

[0010] 0.25-0.5 parts of silicone leveling agent.

[0011] A further improvement of the present invention is:

[0012] The epoxy organosiloxane is one or a mixture of two or more of 3-glycidyloxypropyltrimethoxysilane, 3-glycidyloxypropyltriethoxysilane, diethoxy(3-glycidyloxypropyl)methylsilane, 3-glycidyloxypropylmethyldimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltriethoxysilane, 2-(3,4-epoxycyclohexyl)ethylmethyldiethoxysilane or 5,6-epoxyhexyltriethoxysilane.

[0013] Furthermore, the alkane porogen is one or a mixture of two or more of pentane, hexane, heptane, octane, nonane, decane, dodecane or hexadecane.

[0014] Furthermore, the photoacid generator is one or a mixture of two or more of bis(dodecylphenyl)iodonium hexafluorophosphate, bis(dodecylbenzene)iodonium hexafluoroantimonate, 4-octyloxydiphenyliodonium hexafluoroantimonate or 2-methyl-α-[2-[[propanesulfonyl]imide]-3(2H)-thienylethylene-phenylacetonitrile.

[0015] Furthermore, the organic silicon leveling agent is BYK333 polyether modified organic silicon.

[0016] Furthermore, the substrate material is selected from glass, PMMA, and PVC.

[0017] A further improvement of the present invention is:

[0018] An organosilicon anti-reflection coating is formed by coating the above-mentioned organosilicon anti-reflection coating on a base material and then photocuring it.

[0019] A further improvement of the present invention is:

[0020] A method for preparing an organosilicon anti-reflective coating, characterized in that it comprises the following steps: weighing a certain amount of epoxy organosiloxane, an alkane porogen, a photoacid generator and an organosilicon leveling agent and placing them in a brown glass bottle, stirring in the dark, and after mixing evenly, coating the coating solution on a base material, and irradiating the material with light for 10-30 minutes at a certain temperature to obtain an anti-reflective coating.

[0021] Furthermore, the illumination temperature is 10°C-60°C.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] 1. The present invention selects a dual-functionalized organosilicon precursor of an alkoxysilane group and an epoxy group, and prepares it into a solution with an alkane porogen, a photoacid generator and an organosilicon leveling agent. Under ultraviolet light irradiation, the photoacid generator decomposes to produce a superacid, and simultaneously initiates the hydrolysis and polycondensation of the siloxane group and the cationic polymerization of the epoxy group to form an organosilicon polymer, which is separated from the alkane phase and forms a porous organosilicon bulk polymer coating after volatilization, which has the characteristics of high light transmittance and good anti-reflection performance.

[0024] 2. The porous organosilicon bulk polymer coating formed by the present invention, the inorganic polysiloxane thereof can not only improve the adhesion between the coating and substrate materials such as glass, but also enhance the hardness of the coating; and the polymer molecular chains formed by the polymerization of epoxy groups can provide flexibility for the coating, thereby cooperating with the inorganic polysiloxane molecular chains to provide the coating with excellent mechanical properties.

[0025] 3. The preparation method provided by the present invention utilizes a photoacid generator to simultaneously initiate the hydrolysis and condensation of siloxane groups and the cationic polymerization of epoxy groups under ultraviolet light, and combines the phase separation principle and evaporation mechanism to prepare a porous organosilicon bulk polymer coating in one step. The preparation process is simple and efficient. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 The UV-visible light transmittance curves of the coatings of Example 1 and Example 2 of the present invention are shown;

[0027] Figure 2 The UV-visible light transmittance curves of the coatings of Examples 1 and 3 of the present invention are as follows;

[0028] Figure 3 It is the UV-visible light transmittance curve of the coating of Example 3 and Example 4 of the present invention;

[0029] Figure 4 The UV-visible light transmittance curves of the coatings of Example 1 and Example 5 of the present invention are shown;

[0030] Figure 5The UV-visible light transmittance curves of the coatings of Example 1 and Example 6 of the present invention are shown;

[0031] Figure 6 It is the UV-visible light transmittance curve of the coating of Example 1 and Example 7 of the present invention. DETAILED DESCRIPTION

[0032] The present invention is described in detail below in conjunction with specific embodiments.

[0033] Example 1

[0034] 96.4 parts of 3-glycidyloxypropyltrimethoxysilane, 1.1 parts of n-nonane, 2 parts of bis(dodecylphenyl)iodonium hexafluorophosphate and 0.5 parts of BYK333 polyether-modified silicone were added into a brown glass bottle, stirred for 30 minutes under light-proof conditions, and after uniform mixing, the solution was coated on a glass substrate and irradiated at 20°C for 30 minutes to obtain an anti-reflective coating.

[0035] Example 2

[0036] 96.4 parts of 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, 1.1 parts of n-nonane, 2 parts of bis(dodecylphenyl)iodonium hexafluorophosphate and 0.5 parts of BYK333 polyether-modified silicone were added into a brown glass bottle, stirred for 30 min under light-proof conditions, and after uniform mixing, the solution was coated on a glass substrate and irradiated at 20°C for 30 min to obtain an anti-reflective coating.

[0037] Figure 1 This is a graph of the ultraviolet light transmittance of the coatings of Examples 1 and 2 of the present invention.

[0038] Example 3

[0039] 95.5 parts of 3-glycidyloxypropyltrimethoxysilane, 2 parts of n-nonane, 2 parts of bis(dodecylphenyl)iodonium hexafluorophosphate and 0.5 parts of BYK333 polyether-modified silicone were added into a brown glass bottle, stirred for 30 minutes under light-proof conditions, and after uniform mixing, the solution was coated on a glass substrate and irradiated at 20°C for 30 minutes to obtain an anti-reflective coating.

[0040] Figure 2 This is a data diagram of the anti-reflection performance of the coating obtained in Example 1 and Example 3 of the present invention.

[0041] Example 4

[0042] 95.5 parts of 3-glycidyloxypropyltrimethoxysilane, 2 parts of n-hexadecane, 2 parts of bis(dodecylphenyl)iodonium hexafluorophosphate and 0.5 parts of BYK333 polyether-modified silicone were added into a brown glass bottle, stirred for 30 minutes in a light-proof condition, and after being mixed evenly, the solution was coated on a glass substrate and irradiated at 20°C for 30 minutes to obtain an anti-reflective coating.

[0043] Figure 3 This is a data diagram of the anti-reflection performance of the coating obtained in Examples 3 and 4 of the present invention.

[0044] Example 5

[0045] 96.4 parts of 3-glycidyloxypropyltrimethoxysilane, 1.1 parts of n-nonane, 2 parts of bis(dodecylphenyl)iodonium hexafluorophosphate and 0.5 parts of BYK333 polyether-modified silicone were added into a brown glass bottle, stirred for 30 minutes under light-proof conditions, and after uniform mixing, the solution was coated on a glass substrate and irradiated at 50° C. for 30 minutes to obtain an anti-reflective coating.

[0046] Figure 4 These are the anti-reflection performance data of the coatings obtained after Example 1 and Example 5 of the present invention.

[0047] Example 6

[0048] 96.4 parts of 3-glycidyloxypropyltrimethoxysilane, 1.1 parts of n-nonane, 2 parts of 2-methyl-α-[2-[[propanesulfonyl]imide]-3(2H)-thienyl-phenylacetonitrile and 0.5 parts of BYK333 polyether-modified silicone were added into a brown glass bottle, stirred for 30 minutes under light-proof conditions, and after uniform mixing, the solution was coated on a glass substrate and irradiated at 20°C for 30 minutes to obtain an anti-reflection coating.

[0049] Figure 5 These are the anti-reflection performance data of the coatings obtained after Example 1 and Example 6 of the present invention.

[0050] Example 7

[0051] 94.4 parts of 3-glycidyloxypropyltrimethoxysilane, 1.1 parts of n-nonane, 4 parts of bis(dodecylphenyl)iodonium hexafluorophosphate and 0.5 parts of BYK333 polyether-modified silicone were added into a brown glass bottle, stirred for 30 minutes under light-proof conditions, and after uniform mixing, the solution was coated on a glass substrate and irradiated at 20°C for 30 minutes to obtain an anti-reflective coating.

[0052] Figure 6 These are the anti-reflection performance data of the coatings obtained after Example 1 and Example 7 of the present invention.

[0053] The anti-reflection coatings prepared in Examples 1 to 7 were tested for pencil hardness and adhesion, and the testing methods or standards were as follows:

[0054] Pencil hardness performance test: carried out in accordance with national standard GB / T 6739-2022.

[0055] Adhesion test: in accordance with national standard GB / T 9286-2021

[0056] The pencil hardness and adhesion test results of the products obtained in Examples 1 to 7 are shown in the following table.

[0057]

[0058] The above embodiments are only for illustrating the technical concept and features of the present invention, and their purpose is to enable people familiar with the technology to understand the content of the present invention and implement it accordingly, and they cannot be used to limit the protection scope of the present invention. Any equivalent transformation or modification made according to the spirit of the present invention should be included in the protection scope of the present invention.

Claims

1. An organosilicon anti-reflection coating, characterized in that: The organic silicon anti-reflection coating is formed by coating the organic silicon anti-reflection coating on a base material and then curing the coating with light. The organic silicon anti-reflection coating is composed of the following raw materials in parts by weight: Epoxy organosilane 90-97 parts; 0.2-3 parts of alkane porogen; 1-8 parts of photoacid generator; 0.25-0.5 parts of silicone leveling agent.

2. The organosilicon anti-reflection coating according to claim 1, characterized in that: The epoxy organosiloxane is one or a mixture of two or more of 3-glycidyloxypropyltrimethoxysilane, 3-glycidyloxypropyltriethoxysilane, diethoxy(3-glycidyloxypropyl)methylsilane, 3-glycidyloxypropylmethyldimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltriethoxysilane, 2-(3,4-epoxycyclohexyl)ethylmethyldiethoxysilane or 5,6-epoxyhexyltriethoxysilane.

3. The organosilicon anti-reflection coating according to claim 1, characterized in that: The alkane porogen is one or a mixture of two or more of pentane, hexane, heptane, octane, nonane, decane, dodecane or hexadecane.

4. The organosilicon anti-reflection coating according to claim 1, characterized in that: The photoacid generator is one or a mixture of two or more of bis(dodecylphenyl)iodonium hexafluorophosphate, bis(dodecylbenzene)iodonium hexafluoroantimonate, 4-octyloxydiphenyliodonium hexafluoroantimonate or 2-methyl-α-[2-[[propanesulfonyl]imide]-3(2H)-thienylethylene-phenylacetonitrile.

5. The organosilicon anti-reflection coating according to claim 1, characterized in that: The organic silicon leveling agent is BYK333 polyether modified organic silicon.

6. The organosilicon anti-reflection coating according to claim 1, characterized in that: The substrate material is selected from one of glass, PMMA and PVC.

7. The method for preparing an organosilicon anti-reflective coating according to any one of claims 1 to 6, characterized in that: The following steps are involved: Weigh a certain amount of epoxy organosiloxane, alkane porogen, photoacid generator and silicone leveling agent into a brown glass bottle, stir in the dark, mix evenly, apply the coating solution on the base material, and irradiate with light for 10-30 minutes at a certain temperature to obtain an anti-reflective coating.

8. The method for preparing an organosilicon anti-reflection coating according to claim 7, characterized in that: The light temperature is 10℃-60℃.

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